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Hydrazine hydrate (1:1) → (2R,3R,4R)-1-(2-aminoethyl)-3,4-dibenzyloxy-2-benzyloxymethylpyrrolidine

HRID 1459650
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HRID 1459650 반응식
[CH2:1]([O:8][C@H:9]1[C@H:13]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:12][N:11]([CH2:22][CH2:23][N:24]2C(=O)C3=CC=CC=C3C2=O)[C@@H:10]1[CH2:35][O:36][CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN>C(O)C>[NH2:24][CH2:23][CH2:22][N:11]1[CH2:12][C@@H:13]([O:14][CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C@H:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C@H:10]1[CH2:35][O:36][CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 54238591(2R,3R,4R)-3,4-dibenzyloxy-2-benzyloxymethyl-1-(2-phthalimidoethyl)pyrrolidine2회

생성물 1

HCID 54168326(2R,3R,4R)-1-(2-aminoethyl)-3,4-dibenzyloxy-2-benzyloxymethylpyrrolidine수율 3.1%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

(2R,3R,4R)-3,4-Dibenzyloxy-2-benzyloxymethyl-1-(2-phthal-imidoethyl)pyrrolidine (Compound 19) (0.64 g, 1.1mmol) was dissolved in ethanol (20 ml) and hydrazin, hydrate (0.215 ml, 4.4 mmol) was added. The clear solution was stirred for 4 hours at 40° C. and for 18 hours at room temperature. The white precipitate was filtered off and the filtrate evaporated in vacuo. The residue was partitioned between aqueous hydrochloric acid and methylene chloride. The water phase adjusted to pH 11with 2N sodium hydroxide and extracted with methylene chloride (2×100 ml) and with diethylether (100 ml). Drying of the combined organic phases with magnesium sulphate and evaporation of the solvent in vacuo afforded the crude product as an oil. Purification on silica gel (Eluent: Ethyl acetate) gave (2R,3R,4R)-1-(2-aminoethyl)-3,4-dibenzyloxy-2-benzyloxymethylpyrrolidine (0.015 g) as an oil.

후처리

  1. filtrationThe white precipitate was filtered off
  2. customthe filtrate evaporated in vacuo
  3. customThe residue was partitioned between aqueous hydrochloric acid and methylene chloride
  4. extractionextracted with methylene chloride (2×100 ml) and with diethylether (100 ml)
  5. dry with materialDrying of the combined organic phases with magnesium sulphate and evaporation of the solvent in vacuo
  6. customafforded the crude product as an oil
  7. customPurification on silica gel (Eluent: Ethyl acetate)

출처 및 근거

ORD 기록
ord-44d3b7c511ec4a8ab98e7c5c215e74f1
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05854272

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